微波消解-电感耦合等离子体质谱法测定有机硅树脂中痕量铂元素
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摘要
将微波消解法与电感耦合等离子体质谱(ICP-MS)相结合,通过对微波消解条件及ICP-MS测定条件进行优化,建立了微波消解-电感耦合等离子体质谱法测定有机硅树脂中痕量铂的方法,并对方法的检出限、加标回收率和精密度进行了分析.实验表明:该方法线性范围宽,线性相关系数大于0.9999,方法检出限为0.024μg/L,加标回收率在86.40%～111.74%之间,相对标准偏差小于2.0%.该方法简便、快速、准确,完全能够满足有机硅树脂中铂含量的检测要求.
In this paper,microwave digestion and inductively coupled plasma mass spectrometry (ICP-MS) are applied to determine trace platinum in silicon resin using optimized determination conditions of microwave digestion and ICP-MS,the detection limit,recovery rate and precision of the method are analyzed.The results show that the method gives high linear correlation coefficient with more than 0.9999 in wide linear range,the detection limit is 0.024μg/L,the recoveries rate is in 86.40%～111.74%,and the precision is fine,the relative standard deviation is lower than 2.0%.This method is simple,fast,accurate,and can fully meet the detection requirements of platinum in silicon resin.
In this paper,microwave digestion and inductively coupled plasma mass spectrometry (ICP-MS) are applied to determine trace platinum in silicon resin using optimized determination conditions of microwave digestion and ICP-MS,the detection limit,recovery rate and precision of the method are analyzed.The results show that the method gives high linear correlation coefficient with more than 0.9999 in wide linear range,the detection limit is 0.024μg/L,the recoveries rate is in 86.40%～111.74%,and the precision is fine,the relative standard deviation is lower than 2.0%.This method is simple,fast,accurate,and can fully meet the detection requirements of platinum in silicon resin.
引文
[1]赵陈超,章基凯.有机硅树脂及其应用[M].北京:化学工业出版社,2016:1-17.
[2]中国石油化工总公司.中华人民共和国石油化工行业标准:重整催化剂铂含量测定法:SH/T0570-93[S].北京:中国石化出版社,2004.
[3]李欣,刘月银,景小兵,等.铂-偶氮氯膦-PA-高碘酸钾催化分光光度法测定微量铂[J].应用化学,2003,20(10):1000-1002.
[4]单玲,李俊花,刘树文.用原子吸收光谱法测定催化剂中的Pt含量[J].石油大学学报:自然科学版,2004,28(6):120-122.
[5]王杉,密捷波,李元宗,等.电感耦合等离子体发射光谱测定血清及组织中铂类药物[J].分析化学研究报告,2003,31(3):287-291.
[6]杨丽飞,李异,苏明跃.D290树脂-活性炭吸附电感耦合等离子体原子发射光谱法测定铬精矿中金铂钯[J].冶金分析,2010,30(6):12-15.
[7]孙红林,王琳,陈浩凤,等.电感耦合等离子体原子发射光谱法测定地质样品中铂钯金[J].冶金分析,2015,35(11):8-15.
[8]冯先进,屈太原.电感耦合等离子体质谱法(ICP-MS)最新应用进展[J].中国无机分析化学,2011,1(1):46-52.
[9]陈丽琼,胡勇.电感耦合等离子体质谱法在环境监测中的应用[J].环境科学导刊,2007,26(6):85-88.
[2]中国石油化工总公司.中华人民共和国石油化工行业标准:重整催化剂铂含量测定法:SH/T0570-93[S].北京:中国石化出版社,2004.
[3]李欣,刘月银,景小兵,等.铂-偶氮氯膦-PA-高碘酸钾催化分光光度法测定微量铂[J].应用化学,2003,20(10):1000-1002.
[4]单玲,李俊花,刘树文.用原子吸收光谱法测定催化剂中的Pt含量[J].石油大学学报:自然科学版,2004,28(6):120-122.
[5]王杉,密捷波,李元宗,等.电感耦合等离子体发射光谱测定血清及组织中铂类药物[J].分析化学研究报告,2003,31(3):287-291.
[6]杨丽飞,李异,苏明跃.D290树脂-活性炭吸附电感耦合等离子体原子发射光谱法测定铬精矿中金铂钯[J].冶金分析,2010,30(6):12-15.
[7]孙红林,王琳,陈浩凤,等.电感耦合等离子体原子发射光谱法测定地质样品中铂钯金[J].冶金分析,2015,35(11):8-15.
[8]冯先进,屈太原.电感耦合等离子体质谱法(ICP-MS)最新应用进展[J].中国无机分析化学,2011,1(1):46-52.
[9]陈丽琼,胡勇.电感耦合等离子体质谱法在环境监测中的应用[J].环境科学导刊,2007,26(6):85-88.